Alloy and process of producing the same.



JES 1B. GRENAGLE, 0F CATONSVILLJE, MARYLAND.

ALLUY nine.

Ito Drawing.

prises as a new article an alloy comprising zirconium and iron, saidalloy containing advantageously between and 90 per cent. of zirconiumwith the residue mainly iron, or an iron group metal, and said alloyalso advantageously comprising a certain amount of titanium and alsocomprising in certain cases a small amount of aluminum or other metal;and it also comprises a filament or other luminescent body composed ofsaid al- 10y and it further comprises a method of producing such alloyswherein zirconium and iron compounds are co-reduced in the presence' ofsufiicient titanium compounds to produce certain advantageous efiectsand to insure the entry of 'asmall amount of metallic titanium into thealloy produced; all as more fully hereinafter set forth and as claimed.

Numerous attempts have been made to obtain alloys of zirconium whichcould be worked up into forms commercially useful,

but such attempts have been heretofore largely unsuccessful. Zirconiumitself is a hard, brittle substance existing in several allotropicforms, all of which are easlly fractured and possess little or noductillity or malleability. These properties have also characterizedpractically all the alloys or metal mixtures heretofore produced inwhich zirconium was present in more than comparatively smallproportions. Moreover it' has been found extremely dificult to alloyzirconium with other metals by direct addition of the one metal to theother with production of uniform and homogeneous ductile and malleablealloyed products;

products which are susceptible of being treated by metal-workingprocesses such as drawing, forging, rolling, casting and the like. Thephysical and chemical properties of these dlrectly produced alloysprevent such manipulation.

Accordin to the present invention true alloys of zirconiumwith .iron, oranother Specification oi Letters Patent.

\ PROCESS OF PRODUCING THE SE.

]Patented Dec. d, it 5..

Application filed December 7, 1915. Serial Ito. 55,555.

metal of the iron family, are produced by the simultaneous reduction ofthe constituent metals from compounds containing them. Under theseconditions the zirconium and the iron group metals readily unite .toform homogeneous alloys of varying composltlon depending upon therelativequantities of the materials employed and the conditionsofreduction. The alloys thus produced are of a type hitherto unknown amongmetalhc zlrconium combinations- They exhibit practically no tendency tooxidize and are highly resistant to most chemical reagents. Inappearance they are truly metalllc, and they can be produced in compactbodies which upon grinding and polishing, exhibit bright metallicsurfaces of a silvery steel-like luster. Alloys may be produced'whichare tough and are malleable They possess a remarkably high degree ofluminescence at relatively low filament tem-- peratures andare thus veryefficient sources of light. While other metals of the iron group thaniron itself, such as nickel, cobalt,- or manganese, or alloys ormixtures thereof, are capable of use in the present invention, they arenot in practice as desirable as iron. For the present purposes, iron isby far the most satisfactory metal of the iron group.- The relativeproportions of iron and zirconium in alloys under the present inventionmay vary widely. For most purposes it is desirable to have proportions wich will give alloys which are malleable and ductile, or have goodtensile strength. For binary zirconium-iron alloys, the proportion ofzirconium should not fall much below, say 40 per cent. or thereabout,since with lower percentages of this metal the advantageous propertiesof the alloys are not suiiiciently in evidence. ,Higher percentages ofzirconium in such binary alloys are still more desirable for variousreasons; and the alloys of from approximately 60 to 90 per cent.-zirconium content with to 10 per cent. of iron are particularlyadvantageous.

The excellence of these zirconium alloys may be considerably enhancedand many desirable properties attained by the inclusion of a smallamount of titanium in the alloy, either by co-reduction of titanium withthe other constituents, or by separate addition of titanium to apreformed alloy. The allowable amount of titanium so present is notrigidly restricted, but very small quantities prove efiicacious inpractice. As little as 0.10 per cent. serves the present purpose in someinstances, and it is seldom necessary in alloys for most purposes thatthe titanium content shall exceed 2 or 3 per cent. These small amountsof titanium give enhanced strength and toughness to the zirconiumalloys, and also increase their electrical properties. The ductility andmalleability are also more pronounced. Furthermore in the manufacture ofthese alloys by co-reduction of the component metals, the presence ofthe titanium compounds in the mixture reduced has a useful effect inpreventing the undesirable retention of oxygen and oxygen compounds inthe alloy or resultant melt. The presence of titanium also operates toexclude nitrogen, carbon and other metalloids from the alloy produced.Oxygen and other metalloids have an undesirable effect on malleability,ductility and texture. Ternary alloys containing a certain amount oftitanium with preponderating proportions of zirconium and iron havecertain decided advantages over the simple binary alloys for manypurposes. Finally, the addition of small amounts of other metals such asaluminum, tantalum, columbium, (niobium), etc., give quaternary andstill more complex zirconium-iron alloys which for some purposes ofi'erparticular advantages and in them the relative proportions of zirconiumand iron may often, with advantage, vary more widely than in the simplebinary zirconium iron alloys. It is to be understood, however, that inall these alloys under the present invention the combined zirconium ironcontent preponderates over the other metals. Typical analyses ofquaternary alloys of the present invention comprising zirconium, iron,titanium, and aluminum are as follows: zirconium 65.78%, 8.43%, 32.97%,iron 26.39%, 90.97%, 49.21%, titanium, 0.12%, 0.13%, 0.42%, aluminum7.71%, 0.47%, 17.40%.

The described alloys are substantially iron-zirconium alloys, othermetals forming a minor fraction. And, for practical purposes, thesealloys may be looked upon as zirconium alloyed with iron or itsequivalent, an iron-rich ferrous alloy.

The process of making the described alloys under the present inventionis one of coreduction of compounds containing zirconium and iron in sucha manner that the two metals are presented to each other in a nascentreactive condition. It is best that this reduction occur in the presenceof a titaniferous compound, since as before stated, the inclusion of asmall ercentage of titanium in the alloy prod iiced is especiallyvaluable and the presence of titanium during the reduction is desirablefor the other reasons stated. A convenient method, especially where itis desired to have aluminum present in the alloy, as is often the case,is to reduce mixed oxids of iron and zirconium by means of finelydivided aluminum, the reaction being started With any firing means ormaterials such as magnesium, barium oxids, etc. In making an alloy ofiron and zirconium containin about 44.7 per cent. zirconium thefollowing equation may serve to represent the reaction of reduction byaluminum:

The process of reduction may also be carried out by suitably heating themixed oxids in a graphite crucible as b means of the oxyacetylene flame,or electrlcally. Or, a mixture of titaniferous oxid of iron, and themineral zircon, or other zirconium-containing materials, such aszirconia together with suitable amounts of titaniferous minerals such asrutile, ilmenite, sphene, titanic oxid, etc., may be heated as beforedescribed. Fluxes and slag forming bodies such as silica, soda, etc.,may be employed. The mineral ilmenite is a source of titanium convenientto employ in the present process.

. The alloys thus produced may be mechanically Worked in any suitableway. In making filaments, the alloys, in the form of rods, produced bycasting or by otherwise suitably shaping the alloys produced as abovedescribed may be heated to the necessary temperature, rolled, drawn,swaged or extruded through dies to size, the alloy rod beingconveniently heated by passage of a current therethrough during drawing.With many of the present alloys no special precautions need be taken toavoid oxidation during working, but where necessary or desirable,working may be carried on in vacuo or in an inert atmosphere.

In addition to their utility for incandescent lamp filaments and forglowers, alloys under the present invention may be usefully employed informing arcs. As stated, the present materials give out more light thanis equivalent to their temperature. Being resistant to acids andcorrosion, the alloys may be used for various shaped articles forornamental and other purposes, such as s ark points, etc. Another fieldof utility for t ese alloys is in the manufacture of transformerelements.

was,

Halogen compounds, such as fluorids, chlorids, etc. of the Variousmetals may be used in maklng the alloys by co-reduction; but their useofiers no advantage over the oxidized compounds of the metals asdescribed.

What I claim is 1. As a new article, an alloy comprising not less thanabout 40 per cent. and not more than about 90 per cent. zirconiumtogether with an iron group metal.

2. As a new article, an alloy comprising not less than about 40 percent. and not more than about 90 per cent. zirconium together with iron.I

3. As a new article, an alloy comprising approximately between 60 and 90per cent.

zirconium together with van iron group metal.

4. As a new article, an alloy comprising approximately between 60 and 90per cent.

- zirconium together with iron.

5. An alloy comprising between 60 and 90 per cent. zirconium, theresidue of said alloy being mainly iron, and said alloy beingsubstantially free of oxygen, oxids and metalloids and being malleableand ductile.

6. The process of making an alloy comprising iron and zirconium whichcomprises admixing materials containing compounds of iron and ofzirconium and co-reducing the metals from the mixture as an alloy.

7. llhe process of making an alloy comprising iron and zirconium whichcomprises admixing materials containing compounds of iron, of zirconiumand of titanium and coreducing the metals from the mixture as an alloy.

8. The process of making an alloy comprising iron and zirconium whichcomprises admixing materials containing compounds of iron and ofzirconium with metallic aluminum and igniting the mixture.

In testimon whereof, I afiix my signature in presence 0 two witnesses.

JAMES B. GRENAGLE.

Witnesses:

F. L. MIDDLETON, BENNETT S. Jones.

